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Synthesis Work Full Procedure

This document outlines the detailed synthesis procedures for choline cinnamate ionic liquid from cinnamic acid and choline hydroxide, including required materials and step-by-step instructions. It also describes methods for forming vesicles and gels using the synthesized ionic liquid, detailing necessary materials and procedures for each process. Characterization techniques for both vesicles and gels are mentioned to confirm successful formation.

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dharmeshsaurabh96
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11 views4 pages

Synthesis Work Full Procedure

This document outlines the detailed synthesis procedures for choline cinnamate ionic liquid from cinnamic acid and choline hydroxide, including required materials and step-by-step instructions. It also describes methods for forming vesicles and gels using the synthesized ionic liquid, detailing necessary materials and procedures for each process. Characterization techniques for both vesicles and gels are mentioned to confirm successful formation.

Uploaded by

dharmeshsaurabh96
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Detailed Synthesis Procedure for Choline Cinnamate Ionic Liquid

​ his report provides a comprehensive procedure for synthesizing choline cinnamate ionic liquid
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from cinnamic acid and choline hydroxide (45% solution) using ethanol as a solvent.​

Materials Required:

Reactants:
Cinnamic acid (C₉H₈O₂): 2.948 grams
Choline hydroxide (45% solution): 5.276 grams (total weight before dilution)

Solvent:
Ethanol: 25 mL (15 mL for cinnamic acid solution and 10 mL for choline hydroxide solution)

Equipment:
Round-bottom flask (100 mL)
Magnetic stirrer and stir bar
Beaker for dissolving choline hydroxide
Heating mantle or hot plate
Vacuum system or rotary evaporator
Thermometer
Cooling rack or heat-resistant surface
Sealed storage container

Synthesis Steps
Preparation of Reactant Solutions:
Weigh 2.948 grams of cinnamic acid accurately using an analytical balance.
In a clean round-bottom flask, measure and add 15 mL of ethanol.
Add the cinnamic acid to the flask and stir the mixture at room temperature (25°C) until fully
dissolved, which should take about 5-10 minutes.

Dissolving Choline Hydroxide:


Weigh 5.276 grams of 45% choline hydroxide using the same analytical balance.
In a separate beaker, pour 10 mL of ethanol.
Add the weighed choline hydroxide to the beaker and stir until fully dissolved. This may take a
few minutes, and the solution should be clear.

Combining Solutions:
Once both solutions are ready, slowly add the choline hydroxide solution to the cinnamic acid
solution in the round-bottom flask while stirring continuously.
Ensure to mix thoroughly to promote efficient interaction between the acid and base, aiming for
a single homogenous solution.

Heating the Mixture:


Heat the combined solution to 30°C using a heating mantle or hot plate.
Maintain this temperature for a duration of 2 hours while stirring continuously. This step
facilitates the reaction, allowing the formation of choline cinnamate ionic liquid.

Evaporating the Solvent:


After the stirring period, remove the ethanol solvent using a rotary evaporator or a vacuum
distillation setup. Set the evaporation temperature to 25-30°C to prevent degradation of the
product while ensuring effective solvent removal.
Monitor the process, ensuring that no liquid remains in the flask.

Drying the Ionic Liquid:


Transfer the resultant choline cinnamate into a vacuum drying apparatus.
Dry the product under vacuum at a temperature of 60°C for 24 hours. This step removes any
residual ethanol and enhances the purity of the ionic liquid.

Storage of the Final Product:


Once drying is complete, allow the flask with choline cinnamate to cool to room temperature.
Carefully transfer the ionic liquid into a sealed storage container to protect it from moisture and
light, which may affect its stability.

Detailed Synthesis Procedures for Vesicle and Gel Formation


Using Choline Cinnamate Ionic Liquid

​ his report outlines the synthesis procedures for both vesicles and gel formulations from choline
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cinnamate ionic liquid.​Each procedure includes materials, methods, and conditions necessary
to achieve the desired structures.

I. Synthesis of Vesicles from Choline Cinnamate Ionic Liquid

Materials Required:
Choline cinnamate ionic liquid (from previous synthesis).
Ethanol or water (as solvent).
An amphiphilic surfactant (e.g., lecithin, polyoxyethylene sorbitan monooleate).
Stirring apparatus (magnetic stirrer).
Ultrasonicator or high-shear mixer (for size reduction).
Round-bottom flask or beaker.Appropriate measuring tools and analytical balance.
Procedure:

Preparation of Choline Cinnamate Solution:


Dissolve an appropriate amount of choline cinnamate ionic liquid (e.g., 1 g) in 5 mL of ethanol or
water in a round-bottom flask. The choice of solvent may affect vesicle formation, and a more
hydrophilic solvent may be preferable for stability.

Adding Surfactant:
Add a surfactant such as 0.1 to 0.2 g of lecithin or polyoxyethylene sorbitan monooleate to the
solution.
Stir the mixture at room temperature for 15 minutes until a clear solution forms.

Sonication:
Use an ultrasonicator or high-shear mixer to vigorously mix the solution for 10-20 minutes. This
high-energy mixing method assists in breaking up micelles into smaller vesicles by reducing
their size and promoting self-assembly.

Cooling and Stabilizing:


Allow the mixture to cool to room temperature if heated. This may take 5-10 minutes.
Vesicles can be stabilized by chilling the mixture in an ice bath or keeping it at 4°C for 24 hours
to promote uniform size distribution.

Characterization:
Analyze the vesicle size and structure using dynamic light scattering (DLS) or transmission
electron microscopy (TEM) to confirm successful vesicle formation.

II. Synthesis of Gel from Choline Cinnamate Ionic Liquid

Materials Required:
Choline cinnamate ionic liquid (from previous synthesis).
Suitable gelling agent (e.g., gelatin, xanthan gum, or Alginate).
Deionized water or ethanol (as solvent).
Stirring apparatus (magnetic stirrer).
Heating apparatus (if necessary, for certain gelling agents).
Mold or container for gel formation.

Procedure:

Preparation of Choline Cinnamate Solution:


In a beaker, dissolve 2 to 5 grams of choline cinnamate ionic liquid in 15 mL of deionized water
or ethanol. Ensure complete dissolution by stirring at room temperature for about 10 minutes.
Incorporating the Gelling Agent:
If utilizing gelatin, sprinkle it over the solution to avoid clumping, then allow it to bloom for about
5 minutes. For xanthan gum, slowly add it while stirring vigorously to avoid lumps.
If a heating step is needed (as with gelatin), gently warm the solution to about 40-50°C while
stirring until the gelatin has fully dissolved.

Cooling and Setting the Gel:


After the gelling agent has completely dissolved, remove the heat source and continue stirring.
Pour the mixture into a suitable mold or container and allow it to cool at room temperature for
about 1-2 hours to set the gel. If using reagents that solidify at low temperatures (e.g., gelatin),
place it in a refrigerator for 30 minutes to enhance setting.

Characterization:

Assess gel properties such as texture, appearance, and mechanical integrity. Use rheology to
analyze gel strength and behavior under varying stresses.

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